CN111410199B - White carbon black production device and preparation method - Google Patents
White carbon black production device and preparation method Download PDFInfo
- Publication number
- CN111410199B CN111410199B CN202010378977.2A CN202010378977A CN111410199B CN 111410199 B CN111410199 B CN 111410199B CN 202010378977 A CN202010378977 A CN 202010378977A CN 111410199 B CN111410199 B CN 111410199B
- Authority
- CN
- China
- Prior art keywords
- dispersing
- hollow shaft
- hollow
- film
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000006229 carbon black Substances 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 86
- 238000006243 chemical reaction Methods 0.000 claims abstract description 61
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 43
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 43
- 239000006185 dispersion Substances 0.000 claims abstract description 37
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 19
- 239000012528 membrane Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 29
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 26
- 238000009423 ventilation Methods 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 15
- 239000004115 Sodium Silicate Substances 0.000 claims description 13
- 235000019353 potassium silicate Nutrition 0.000 claims description 13
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 239000012043 crude product Substances 0.000 claims description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims description 10
- 239000003085 diluting agent Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000005543 nano-size silicon particle Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000004537 pulping Methods 0.000 claims description 7
- 238000001694 spray drying Methods 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 5
- 239000012066 reaction slurry Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 description 50
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 229960001866 silicon dioxide Drugs 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 229960004029 silicic acid Drugs 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000010058 rubber compounding Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention provides a production device and a preparation method of white carbon black, comprising the following steps: the device comprises a power device, a reaction kettle, a hollow shaft, a dispersing blade and a dispersing film; the power device is arranged outside the reaction kettle, and the hollow shaft, the dispersing blades and the dispersing film are arranged inside the reaction kettle; the driving shaft of the power device is connected with the hollow shaft to drive the hollow shaft to rotate; the dispersing blades are hollow, and the hollow shafts are connected with the dispersing blades; the dispersing blade is provided with an air outlet hole communicated with the hollow part in the interior, the surface of the dispersing blade is connected with a dispersing film, and one side of the dispersing film, which is clung to the dispersing blade, is communicated with the air outlet hole; the hollow shaft is provided with a shaft air delivery port so as to deliver air to the hollow shaft, the dispersing blades and the dispersing film in sequence through the air delivery port. Carbon dioxide gas required for producing the white carbon black is dispersed through the dispersion membrane and then enters the reaction liquid, a special high-pressure pump is not required for conveying, and the dispersed carbon dioxide can be uniformly dispersed in the reaction liquid by utilizing the rotation of the dispersion blade, so that the production of the white carbon black is facilitated.
Description
Technical Field
The invention relates to the technical field of white carbon black production, in particular to a production device and a preparation method of white carbon black.
Background
White carbon black is a generic term for white powdered X-ray amorphous silicic acid and silicate products, and mainly refers to precipitated silica, fumed silica and ultrafine silica gel, and also includes powdered synthetic aluminum silicate, calcium silicate, and the like. White carbon black is a porous substance, the composition of which can be represented by SiO2.nH2O, wherein nH2O exists in the form of surface hydroxyl groups, and the white carbon black can be dissolved in caustic alkali and hydrofluoric acid, is insoluble in water, solvents and acid (except hydrofluoric acid), and has the advantages of high temperature resistance, incombustibility, no smell and good electrical insulation.
However, the existing production process of white carbon black involves carbon dioxide and needs to mix the carbon dioxide into the reaction liquid, but the existing dispersion method mainly relies on a stirring mode to carry out, and cannot achieve a good mixing effect.
Thus, there is a need for a better white carbon black production scheme.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a production device and a preparation method of white carbon black, carbon dioxide gas required for producing white carbon black is dispersed through a dispersion film and then enters into reaction liquid, a special high-pressure pump is not required for conveying, and the dispersed carbon dioxide can be uniformly dispersed in the reaction liquid by utilizing rotation of a dispersion blade, so that the production of white carbon black is facilitated.
Specifically, the present invention proposes the following specific embodiments:
the embodiment of the invention provides a device for producing white carbon black, which comprises the following components: the device comprises a power device, a reaction kettle, a hollow shaft, a dispersing blade and a dispersing film;
the power device is arranged outside the reaction kettle, and the hollow shaft, the dispersing blades and the dispersing film are all arranged inside the reaction kettle;
the driving shaft of the power device is connected with the hollow shaft so as to drive the hollow shaft to rotate;
the inside of the dispersing blade is hollow, the hollow shaft is connected with the dispersing blade, and the hollow part of the hollow shaft is communicated with the hollow part of the dispersing blade;
the dispersing blades are provided with air outlet holes communicated with the hollow part in the inner part, the surfaces of the dispersing blades are connected with the dispersing films, and one side, which is clung to the dispersing blades, of each dispersing film is communicated with the air outlet holes;
the hollow shaft is provided with a shaft gas transmission port, so that gas is transmitted to the hollow shaft, the dispersing blades and the dispersing film in sequence through the gas transmission port.
In a specific embodiment, the method further comprises: a dispersion plate; the dispersing plate is provided with a plate input port;
the dispersing plate is hollow, and the first surface of the dispersing plate is also provided with air outlet holes communicated with the hollow part inside;
the first surface of the dispersion plate is provided with the dispersion film; the other side of the dispersing plate is fixed on the inner wall of the reaction kettle.
In a specific embodiment, the dispersion film is a multilayer metal sintering mesh.
In a specific embodiment, the filtration accuracy of the dispersion film is between 1 and 50 μm.
In a specific embodiment, the dispersion film is connected to the liquid surface of the dispersion blade.
In a specific embodiment, the method further comprises: a seal box; the sealing box is sleeved on the shaft air conveying port to ensure tightness when the air is conveyed to the hollow shaft.
In a specific embodiment, the method further comprises: a heater; wherein, the heater sets up on the reation kettle for the reation kettle heats.
In a specific embodiment, the heater comprises: heating wires, or steam coils, or jacketed steam heaters.
The embodiment of the invention also provides a method for preparing the white carbon black based on the white carbon black production device, which is applied to the method and comprises the following steps:
injecting water glass diluent into the reaction kettle, and starting a power device to stir and heat;
inputting carbon dioxide into the water glass diluent, controlling the reaction temperature to be between 50 and 90 ℃ and stopping ventilation after the ventilation time is between 5 and 45 minutes;
continuously introducing carbon dioxide gas into the reaction liquid, controlling the reaction temperature to be 70-95 ℃, and stopping ventilation after the ventilation time is between 10 and 45 minutes;
keeping the reaction temperature within the range of 70-95 ℃, starting the power device to stir for 10-150min, and stopping the reaction when the pH value of the reaction solution is controlled to be 5.5-10.0;
filtering and washing the reaction slurry to obtain a crude product, and pulping and spray-drying the crude product to obtain the nano silicon dioxide product.
In a specific embodiment, the waterglass diluent is formulated using a commercial sodium silicate solution having a Baume degree at grade 38, with a modulus in the range of 3-4.
Therefore, the embodiment of the invention provides a production device and a preparation method of white carbon black, wherein the device comprises the following steps: the device comprises a power device, a reaction kettle, a hollow shaft, a dispersing blade and a dispersing film; the power device is arranged outside the reaction kettle, and the hollow shaft, the dispersing blades and the dispersing film are all arranged inside the reaction kettle; the driving shaft of the power device is connected with the hollow shaft so as to drive the hollow shaft to rotate; the inside of the dispersing blade is hollow, the hollow shaft is connected with the dispersing blade, and the hollow part of the hollow shaft is communicated with the hollow part of the dispersing blade; the dispersing blades are provided with air outlet holes communicated with the hollow part in the inner part, the surfaces of the dispersing blades are connected with the dispersing films, and one side, which is clung to the dispersing blades, of each dispersing film is communicated with the air outlet holes; the hollow shaft is provided with a shaft gas transmission port, so that gas is transmitted to the hollow shaft, the dispersing blades and the dispersing film in sequence through the gas transmission port. Carbon dioxide gas required for producing the white carbon black is dispersed through the dispersion membrane and then enters the reaction liquid, a special high-pressure pump is not required for conveying, and the dispersed carbon dioxide can be uniformly dispersed in the reaction liquid by utilizing the rotation of the dispersion blade, so that the production of the white carbon black is facilitated.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a device for producing white carbon black according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a hollow mandrel of a white carbon black production device according to an embodiment of the present invention;
FIG. 3 is a schematic top view of a hollow mandrel of a white carbon black production device according to an embodiment of the present invention;
FIG. 4 is a schematic view of the portion of FIG. 2 A-A;
FIG. 5 is a schematic diagram of a device for producing white carbon black according to an embodiment of the present invention;
FIG. 6 is a schematic structural view of a dispersion plate in a device for producing white carbon black according to an embodiment of the present invention;
fig. 7 is a schematic top view of a dispersing plate in a white carbon black production device according to an embodiment of the present invention;
fig. 8 is a schematic flow chart of a preparation method of white carbon black according to an embodiment of the present invention.
Legend description:
1-a power plant; 2-a reaction kettle; 3-hollow shaft;
4-dispersing blades; 5-a dispersion film; 6-a dispersion plate; 7-sealing the box.
Detailed Description
Hereinafter, various embodiments of the present disclosure will be more fully described. The present disclosure is capable of various embodiments and of modifications and variations therein. However, it should be understood that: there is no intention to limit the various embodiments of the disclosure to the specific embodiments disclosed herein, but rather the disclosure is to be interpreted to cover all modifications, equivalents, and/or alternatives falling within the spirit and scope of the various embodiments of the disclosure.
The terminology used in the various embodiments of the disclosure is for the purpose of describing particular embodiments only and is not intended to be limiting of the various embodiments of the disclosure. As used herein, the singular is intended to include the plural as well, unless the context clearly indicates otherwise. Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which various embodiments of this disclosure belong. The terms (such as those defined in commonly used dictionaries) will be interpreted as having a meaning that is the same as the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein in the various embodiments of the disclosure.
Example 1
The embodiment 1 of the invention provides a white carbon black production device, as shown in fig. 1-7, comprising: the device comprises a power device 1, a reaction kettle 2, a hollow shaft 3, dispersing blades 4 and a dispersing film 5;
the power device 1 is arranged outside the reaction kettle 2, and the hollow shaft 3, the dispersing blades 4 and the dispersing film 5 are all arranged inside the reaction kettle 2;
the driving shaft of the power device 1 is connected with the hollow shaft 3 to drive the hollow shaft 3 to rotate;
as shown in fig. 2 to 4, the inside of the dispersing blade 4 is hollow, the hollow shaft 3 is connected to the dispersing blade 4, and the hollow portion of the hollow shaft 3 is communicated with the hollow portion of the dispersing blade 4;
the dispersing blades 4 are provided with air outlet holes communicated with the hollow part in the interior, the surface of the dispersing blades 4 is connected with the dispersing film 5, and one side, which is clung to the dispersing blades 4, of the dispersing film 5 is communicated with the air outlet holes;
the hollow shaft 3 is provided with a shaft air delivery port so as to sequentially deliver air to the hollow shaft 3, the dispersing blades 4 and the dispersing film 5 through the air delivery port.
The reactor 2 is used for containing reaction liquid, and is a liquid reactor.
The power device 1 is arranged outside the reaction kettle 2 and provides power for the rotation of the hollow shaft 3.
More specifically, the reaction kettle 2 is cylindrical in shape, and the power device 1 is disposed on a central shaft above the reaction kettle 2.
As shown in fig. 1 or fig. 5, the rotation of the hollow shaft 3 drives the dispersing blade 4 to rotate, and the hollow structure inside the hollow shaft 3 can transmit air to the hollow structure of the dispersing blade 4, so that the dispersing film 5 on the dispersing blade 4 can disperse other substances to, for example, a micron level while stirring the liquid, and further, the dispersed carbon dioxide is uniformly dispersed in the reaction liquid.
The hollow shaft 3 can be connected with the dispersing blades 4 at a plurality of positions thereof, so that a plurality of layers of dispersing blades 4 are formed, and a better stirring effect is achieved.
The gas enters the dispersing blades 4 from the hollow shaft 3, and in the rotating state of the dispersing blades 4, the gas is dispersed to reach a micron-sized gas column through the dispersing film 5 and directly enters the liquid-solid mixed phase. The dispersing blade 4 and the mixed liquid are in relative operation, so that the dispersing blade 4 is in a micron-sized layer and uniformly dispersed.
In a specific embodiment, to further uniformly disperse the dispersed carbon dioxide in the reaction solution, the apparatus further includes, as shown in fig. 5: a dispersion plate 6; the dispersion plate 6 is provided with a plate input port;
as shown in fig. 6-7, the dispersing plate 6 is hollow, and the first surface of the dispersing plate 6 is also provided with air outlet holes communicated with the hollow part;
the first surface of the dispersion plate 6 is provided with the dispersion film 5; the other side of the dispersion plate 6 is fixed on the inner wall of the reaction kettle 2.
Specifically, similar to the dispersing blades 4, the dispersing plate 6 has a hollow internal structure and is connected with a plate input port so as to externally input gas, and one surface of the dispersing plate 6 is also provided with a gas outlet hole communicated with the hollow part inside the dispersing plate and communicated with the dispersing film 5, so that the gas is dispersed through the dispersing film 5, and the gas of the reaction liquid is convenient to mix.
The specific dispersion plate 6 may be rectangular.
In a specific embodiment, the dispersion film 5 is a multilayer metal sintering net. Specifically, the multilayer metal sintering net (for example, 5 layers of metal sintering nets) is used as the metal dispersion film, and gas dispersion can be performed more effectively.
Specifically, in a specific embodiment, the filtration accuracy of the dispersion film 5 is any value between 1 and 50 μm, and specific filtration accuracy may be, for example, 1 μm, 2 μm, 3 μm, 5 μm, 7 μm, 10 μm, 15 μm, 17 μm, 20 μm, 22 μm, 23 μm, 25 μm, 27 μm, 30 μm, 35 μm, 37 μm, 40 μm, 45 μm, 47 μm, 50 μm, and so forth.
In a specific embodiment, the dispersing membrane 5 is connected to the liquid surface of the dispersing blade 4 for better gas dispersion.
In a specific embodiment, the apparatus further comprises: a seal box 7; the sealing box 7 is sleeved on the shaft air conveying port so as to ensure the tightness when the air is conveyed to the hollow shaft 3.
Specifically, the effect of transmitting gas to the hollow shaft 3 and preventing leakage is realized through the sealing box 7, so that the air tightness is ensured.
In a specific embodiment, to accelerate the reaction and increase the solubility of the gas in the end of the reaction solution, the apparatus may further include: a heater; wherein, the heater is arranged on the reaction kettle 2 and is used for heating the reaction kettle 2.
Specifically, to facilitate heating, the heater includes: heating wires, or steam coils, or jacketed steam heaters.
In a specific embodiment, the power plant 1 comprises: and a motor. The rotation power is improved by the motor for the hollow shaft 3.
Example 2
The embodiment 2 of the invention also discloses a method for preparing white carbon black based on the white carbon black production device in the embodiment 1, as shown in fig. 8, the method comprises the following steps:
step 101, injecting water glass diluent into the reaction kettle, and starting a power device to stir and heat;
before step 101 is performed, gas outlet holes (may be gas outlet holes on the dispersing film) are already attached to the dispersing blades of the reaction kettle
102, inputting carbon dioxide into water glass diluent, controlling the reaction temperature range between 50 ℃ and 90 ℃ and stopping ventilation after the ventilation time is between 5min and 45 min;
specifically, by opening the carbon dioxide valve, carbon dioxide gas can enter the solution obtained in step 101 from the hollow shaft to the dispersing blade (or carbon dioxide gas can be injected into the solution together with the dispersing blade and the dispersing plate), the reaction temperature is controlled to be 50-90 ℃, the ventilation time is controlled to be 5-45min, and ventilation is stopped.
Step 103, continuously introducing carbon dioxide gas into the reaction liquid, controlling the reaction temperature to be 70-95 ℃, and stopping ventilation after the ventilation time is between 10 and 45 minutes;
specifically, in step 103, carbon dioxide gas is continuously introduced, the reaction temperature is controlled to be 70-95 ℃, the ventilation time is controlled to be 10-45min, and ventilation is stopped.
104, keeping the reaction temperature within the range of 70-95 ℃, starting the power device to stir for 10-150min, and stopping the reaction when the pH value of the reaction solution is controlled to be 5.5-10.0;
step 105, filtering and washing the reaction slurry to obtain a crude product, and pulping and spray-drying the crude product to obtain a nano silicon dioxide product (namely white carbon black).
In a specific embodiment, the water glass diluent of step 101 is formulated using a commercially available sodium silicate solution having a Baume degree in the range of 2.0-4.0, which is a grade 2-38 product.
The device and the corresponding method of the embodiment of the invention prepare the nano silicon dioxide, the nitrogen adsorption specific surface is 180-360 m < 2 >/g, the total pore volume is 1.1-2.0 cm < 3 >/g, the average pore diameter is 5-25 nm, the median particle diameter is 1.0-10 mu m, dV/dlogD (corresponding value at 80nm in nitrogen adsorption data) is less than or equal to 1.8; the product is proved by rubber formula experiments to have better dispersity, excellent reinforcing performance, low abrasion and good wet skid resistance.
Specifically, the present embodiment may have the following different application examples:
application example 1
The preparation method of the white carbon black comprises the following steps:
1) A1 μm dispersion film was attached to the stirring blade of the reaction vessel.
2) Taking sodium silicate solution with the modulus of 3.4 and the commercial Baume degree of 38 grade, and preparing dilute water glass 120L with the Baume degree of 22;
3) Conveying the sodium silicate solution in the step 1) into a 150L reaction kettle through a pump, stirring and heating the liquid, setting the stirring speed to be 12Hz and the temperature to be 70 ℃;
4) When the temperature reaches 70 ℃, opening a carbon dioxide valve, allowing gas to enter the solution through the hollow shaft and the dispersing blades, introducing carbon dioxide gas with the concentration of 100wt%, and simultaneously improving the stirring speed to 20Hz;
5) After introducing carbon dioxide gas for 28min, stopping ventilation, and setting the temperature to 90 ℃;
6) After the temperature was increased to 90 ℃, the carbon dioxide valve was opened again, and carbon dioxide gas with a concentration of 100wt% was introduced for 17 minutes at a stirring speed of 38Hz.
7) Introducing carbon dioxide gas for 115min, stopping ventilation, and simultaneously taking a small amount of reaction liquid, and measuring the pH value of the reaction liquid, wherein the pH value is 8.1;
8) The slurry obtained in step 7) was filtered with a filter press and washed with water, and when the washing liquid had a conductivity of 1100. Mu.s/cm, the washing was stopped, whereupon a cake was obtained as a crude silica product.
9) Pulping the crude product obtained in the step 8), and performing spray drying to obtain a nano silicon dioxide product.
The product detection index is shown in table 1.
Application example 2
The preparation method of the white carbon black comprises the following steps:
1) A dispersing film of 5 μm was attached to the stirring blade of the reaction vessel.
2) Taking sodium silicate solution with the modulus of 3.2 and the commercial Baume degree of 38 grade, and preparing dilute water glass 120L with the Baume degree of 25;
3) Conveying the sodium silicate solution in the step 2) into a 150L reaction kettle through a pump, opening stirring and heating the liquid, setting the stirring speed to be 12Hz and the temperature to be 70 ℃;
4) When the temperature reaches 70 ℃, opening a carbon dioxide valve, allowing gas to enter the solution through the hollow shaft and the dispersing blades, introducing carbon dioxide gas with the concentration of 100wt%, and simultaneously improving the stirring speed to 20Hz;
5) After introducing carbon dioxide gas for 20min, stopping ventilation, and setting the temperature to 90 ℃;
6) After the temperature was increased to 90 ℃, the carbon dioxide valve was opened again, and carbon dioxide gas with a concentration of 100wt% was introduced for 25 minutes at a stirring speed of 38Hz.
7) Introducing carbon dioxide gas for 110min, stopping ventilation, and simultaneously taking a small amount of reaction liquid, and measuring the pH value of the reaction liquid, wherein the pH value is 8.3;
8) The slurry obtained in step 7) was filtered with a filter press and washed with hot water, and when the washing liquid had an electrical conductivity of 1100. Mu.s/cm, the washing was stopped, whereupon a filter cake was obtained as a crude silica product.
9) Pulping the crude product obtained in the step 8), and performing spray drying to obtain a nano silicon dioxide product.
The product detection index is shown in table 1.
Application example 3
The preparation method of the white carbon black comprises the following steps:
1) A20 μm dispersion film was attached to the stirring blade of the reaction vessel.
2) Taking sodium silicate solution of a first grade product with the modulus of 3.3 and the commercial Baume degree of about 38, and preparing the sodium silicate solution into diluted water glass 120L with the Baume degree of 16;
3) Conveying the sodium silicate solution in the step 2) into a 150L reaction kettle through a pump, stirring and heating the liquid, setting the stirring speed to be 12Hz and the temperature to be 70 ℃;
4) When the temperature reaches 70 ℃, opening a carbon dioxide valve, allowing gas to enter the solution through the hollow shaft and the dispersing blades, introducing carbon dioxide gas with the concentration of 100wt%, and simultaneously improving the stirring speed to 20Hz;
5) After introducing carbon dioxide gas for 20min, stopping ventilation, and setting the temperature to 90 ℃;
6) After the temperature is increased to 90 ℃, the carbon dioxide valve is opened again, carbon dioxide gas with the concentration of 100wt% is introduced, the time is 20min, and the stirring speed is increased to 38Hz.
7) Introducing carbon dioxide gas for 95min, stopping ventilation, and simultaneously taking a small amount of reaction liquid, and measuring the pH value of the reaction liquid, wherein the pH value is 8.3;
8) The slurry obtained in step 7) was filtered with a filter press and washed with hot water, and when the washing liquid had an electrical conductivity of 1100. Mu.s/cm, the washing was stopped, whereupon a filter cake was obtained as a crude silica product.
9) Pulping the crude product obtained in the step 8), and performing spray drying to obtain a nano silicon dioxide product.
The product detection index is shown in table 1.
Comparative application example 1
The difference from application example 1 is that the stirring device of the reaction kettle is a stirring paddle for general industry, and the upper end cover of the reaction kettle is provided with a vent pipe device.
The preparation method comprises the following steps:
1) Taking sodium silicate solution with the modulus of 3.4 and the commercial Baume degree of 38 grade, and preparing dilute water glass 120L with the Baume degree of 22;
2) Conveying the sodium silicate solution in the step 2) into a 150L reaction kettle through a pump, stirring and heating the liquid, setting the stirring speed to be 12Hz and the temperature to be 70 ℃;
3) When the temperature reaches 70 ℃, opening a carbon dioxide valve, introducing gas into the solution, introducing carbon dioxide gas with the concentration of 100wt%, and simultaneously improving the stirring speed to 20Hz;
4) After introducing carbon dioxide gas for 160min, stopping ventilation;
5) The slurry obtained in step 4) was filtered with a filter press and washed with hot water, and when the washing liquid had an electrical conductivity of 1100. Mu.s/cm, the washing was stopped, whereupon a filter cake was obtained as a crude silica product.
6) Pulping the crude product obtained in the step 5), and performing spray drying to obtain a nano silicon dioxide product.
7) The product detection index is shown in table 1.
The test data for the nano-silica products prepared in comparative application example 1 are shown in Table 1.
TABLE 1 detection data for products of application examples 1-3 and comparative application example 1
Note that: 1) Nitrogen adsorption specific surface area NSA determination was according to: according to GB/T10722-2014 carbon black total surface area and external surface area determination;
2) CTAB specific surface area measurement was performed in accordance with: determination of specific surface area of precipitated hydrated silica according to GB/T23656-2009 rubber compounding agent.
3) DBP assay was performed according to: determination of the oil absorption value of precipitated hydrated silica according to HG/T3072-2008 rubber compounding agent.
4) Average pore size was determined according to: measurement of the average pore size of precipitated hydrated silica of GB/T28600-2012 rubber compounding agent.
5) dV/dlogD value: in the nitrogen adsorption data, the corresponding values at 80nm were obtained.
6) Median particle size D50 determination is in accordance with: determination of the particle size distribution of the precipitated hydrated silica of the GB/T32698-2016 rubber compounding agent.
As can be seen from Table 1, the scheme corresponding to the present application is significantly better than the conventional scheme at present, the present invention utilizes the characteristics of the membrane and the gas to disperse the gas to the micron level, the gas and the liquid are mixed in the reaction vessel through the dispersing blade, and the local turbulence and the micron level laminar flow are formed at the thin surface parallel to the dispersing blade, so that the carbon dioxide can be uniformly dispersed in the solution, and the reaction efficiency can be greatly improved. The method comprises the following steps: the dispersing blades are provided with dispersing films, carbon dioxide gas enters the blades from the hollow shafts, and in the rotating state of the dispersing blades, the gas enters the solution after reaching a micron-sized gas column after being dispersed through the dispersing films, so that the dispersing blades close to the dispersing films are uniformly dispersed in a micron-sized layer, and the whole solution is in radial flow and axial flow in the reactor, so that the reacted slurry is uniformly mixed; furthermore, the invention can reasonably control the carbonization reaction steps, including setting multiple carbonization steps, reasonably controlling the reaction temperature and ventilation time of each carbonization step, and dispersing the film to avoid the problems of equipment blockage and the like.
Those skilled in the art will appreciate that the drawing is merely a schematic illustration of a preferred implementation scenario and that the modules or flows in the drawing are not necessarily required to practice the invention.
Those skilled in the art will appreciate that modules in an apparatus in an implementation scenario may be distributed in an apparatus in an implementation scenario according to an implementation scenario description, or that corresponding changes may be located in one or more apparatuses different from the implementation scenario. The modules of the implementation scenario may be combined into one module, or may be further split into a plurality of sub-modules.
The above-mentioned inventive sequence numbers are merely for description and do not represent advantages or disadvantages of the implementation scenario.
The foregoing disclosure is merely illustrative of some embodiments of the invention, and the invention is not limited thereto, as modifications may be made by those skilled in the art without departing from the scope of the invention.
Claims (6)
1. The white carbon black production device is characterized by comprising: the device comprises a power device, a reaction kettle, a hollow shaft, a dispersing blade and a dispersing film;
the power device is arranged outside the reaction kettle, and the hollow shaft, the dispersing blades and the dispersing film are all arranged inside the reaction kettle;
the driving shaft of the power device is connected with the hollow shaft so as to drive the hollow shaft to rotate;
the inside of the dispersing blade is hollow, the hollow shaft is connected with the dispersing blade, and the hollow part of the hollow shaft is communicated with the hollow part of the dispersing blade;
the dispersing blades are provided with air outlet holes communicated with the hollow part in the inner part, the surfaces of the dispersing blades are connected with the dispersing films, and one side, which is clung to the dispersing blades, of each dispersing film is communicated with the air outlet holes;
a shaft gas transmission port is arranged on the hollow shaft to transmit gas to the hollow shaft, the dispersing blades and the dispersing film in sequence through the gas transmission port;
further comprises: a dispersion plate; the dispersing plate is provided with a plate input port;
the dispersing plate is hollow, and the first surface of the dispersing plate is also provided with air outlet holes communicated with the hollow part inside;
the first surface of the dispersion plate is provided with the dispersion film; the other surface of the dispersing plate is fixed on the inner wall of the reaction kettle;
the dispersion film is connected to the liquid facing surface of the dispersion blade;
further comprises: a seal box; the sealing box is sleeved on the shaft air conveying port so as to ensure the tightness when the air is conveyed to the hollow shaft;
further comprises: a heater; wherein, the heater sets up on the reation kettle for the reation kettle heats.
2. The apparatus of claim 1, wherein the dispersion film is a multilayer metal sintered mesh.
3. The device of claim 1, wherein the dispersion membrane has a filtration accuracy of between 1 and 50 μm.
4. The apparatus of claim 1, wherein the heater comprises: heating wires, or steam coils, or jacketed steam heaters.
5. A method for preparing white carbon black based on the white carbon black production device of any one of claims 1 to 4, comprising the steps of:
injecting water glass diluent into the reaction kettle, and starting a power device to stir and heat;
inputting carbon dioxide into the water glass diluent, controlling the reaction temperature to be between 50 and 90 ℃ and stopping ventilation after the ventilation time is between 5 and 45 minutes;
continuously introducing carbon dioxide gas into the reaction liquid, controlling the reaction temperature to be 70-95 ℃, and stopping ventilation after the ventilation time is between 10 and 45 minutes;
keeping the reaction temperature within the range of 70-95 ℃, starting the power device to stir for 10-150min, and stopping the reaction when the pH value of the reaction solution is controlled to be 5.5-10.0;
filtering and washing the reaction slurry to obtain a crude product, and pulping and spray-drying the crude product to obtain the nano silicon dioxide product.
6. The method for preparing white carbon black according to claim 5, wherein the water glass diluent is prepared by using a sodium silicate solution of grade 38 commercial sodium silicate with a modulus ranging from 3 to 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010378977.2A CN111410199B (en) | 2020-05-07 | 2020-05-07 | White carbon black production device and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010378977.2A CN111410199B (en) | 2020-05-07 | 2020-05-07 | White carbon black production device and preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111410199A CN111410199A (en) | 2020-07-14 |
| CN111410199B true CN111410199B (en) | 2024-03-22 |
Family
ID=71487129
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010378977.2A Active CN111410199B (en) | 2020-05-07 | 2020-05-07 | White carbon black production device and preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111410199B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1368271A1 (en) * | 1985-11-27 | 1988-01-23 | Всесоюзный Научно-Исследовательский Институт Водоснабжения,Канализации,Гидротехнических Сооружений И Инженерной Гидрогеологии | Device for dispersing gas in liquid |
| CN1143912A (en) * | 1994-03-16 | 1997-02-26 | 普罗迪法股份有限公司 | Dynamic dispenser for substance such as perfume |
| CN2613482Y (en) * | 2003-04-03 | 2004-04-28 | 西安交通大学 | Aeration stirring device |
| CN106673223A (en) * | 2017-01-16 | 2017-05-17 | 四川理工学院 | Aeration device based on turbulent microbubbles |
| CN208894199U (en) * | 2018-06-27 | 2019-05-24 | 怡维怡橡胶研究院有限公司 | A kind of precipitated silica generating device |
| CN212356558U (en) * | 2020-05-07 | 2021-01-15 | 江苏麒祥高新材料有限公司 | White carbon black production device |
-
2020
- 2020-05-07 CN CN202010378977.2A patent/CN111410199B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1368271A1 (en) * | 1985-11-27 | 1988-01-23 | Всесоюзный Научно-Исследовательский Институт Водоснабжения,Канализации,Гидротехнических Сооружений И Инженерной Гидрогеологии | Device for dispersing gas in liquid |
| CN1143912A (en) * | 1994-03-16 | 1997-02-26 | 普罗迪法股份有限公司 | Dynamic dispenser for substance such as perfume |
| CN2613482Y (en) * | 2003-04-03 | 2004-04-28 | 西安交通大学 | Aeration stirring device |
| CN106673223A (en) * | 2017-01-16 | 2017-05-17 | 四川理工学院 | Aeration device based on turbulent microbubbles |
| CN208894199U (en) * | 2018-06-27 | 2019-05-24 | 怡维怡橡胶研究院有限公司 | A kind of precipitated silica generating device |
| CN212356558U (en) * | 2020-05-07 | 2021-01-15 | 江苏麒祥高新材料有限公司 | White carbon black production device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111410199A (en) | 2020-07-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100463851C (en) | Method for preparing super fine hydrophobic silicon dioxide | |
| CN204973893U (en) | Nanometer brium carbonate carbonization reaction unit | |
| CN104016391A (en) | Method for preparing nanometer calcium carbonate for organic silicone electronic sealant by adopting continuous carbonization device | |
| CN111440358B (en) | Nano silicon dioxide for rubber reinforcement and preparation method thereof | |
| CN111410199B (en) | White carbon black production device and preparation method | |
| CN106115754A (en) | A kind of method preparing transparent aluminium hydroxide liquid dispersion | |
| CN106554643B (en) | The preparation method of high temperature resistant bismuth vanadium pigments | |
| CN106943911A (en) | A kind of building coating process equipment | |
| CN110449133A (en) | Chitosan/silicon dioxide composite material | |
| CN105271194B (en) | A kind of preparation method of the graphene quantum dot containing methoxyl group | |
| CN102372274B (en) | Preparation method for bifunctional-modified montmorillonite dispersion liquid | |
| CN106422826A (en) | Uniform mixing and stirring apparatus of pesticide emulsion containing surfactant | |
| CN106315593A (en) | Preparation method for ultra-micropore nanometer SiO2 | |
| CN103360798A (en) | Method for preparing hydrophobic white carbon black | |
| WO2023213069A1 (en) | Preparation process for modified polyamide wax for coatings, and coating formed thereby | |
| CN112111180A (en) | Production process of low-viscosity iron oxide yellow | |
| CN212356558U (en) | White carbon black production device | |
| CN111471344B (en) | Silicon dioxide matting powder and preparation method thereof | |
| CN107824077A (en) | Dispersion impeller component, super effect are stirred dispersion machine and continuous reaction system | |
| CN210332670U (en) | Filter pressing equipment with hydrolysis and washing functions | |
| CN216359017U (en) | Device for preparing calcium-silicon core-shell structure nano calcium carbonate | |
| CN109205630B (en) | Preparation method of monodisperse nano-silicon dioxide transparent dispersoid | |
| CN207042475U (en) | A kind of dynamic pipe reaction device for preparing micro-nano powder | |
| CN110951359A (en) | High-strength water-based automobile coating, preparation method and equipment | |
| CN220520156U (en) | Device for purifying carbon nano tube powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |